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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >Azo coupling-based derivatization method for high-sensitivity liquid chromatography-tandem mass spectrometry analysis of tetrahydrocannabinol and other aromatic compounds
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Azo coupling-based derivatization method for high-sensitivity liquid chromatography-tandem mass spectrometry analysis of tetrahydrocannabinol and other aromatic compounds

机译：基于AZO耦合的衍生衍生化方法，用于高灵敏度液相色谱 - 串联质谱分析，四氢尼醇和其它芳族化合物

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摘要

An azo coupling-based derivatization method is reported for high-sensitivity liquid chromatography-tandem mass spectrometry (LC-MS/MS) quantitation of tetrahydrocannabinol (THC) and other aromatic compounds, i.e. phenols and amines. Through the azo coupling of a diazonium to an analyte, it produces a derivatized analyte which has enhanced ionization efficiency and results in high-response fragments in tandem mass spectrometry. The derivatization method was applied to six typical aromatic compounds using three different diazonium salts as derivatization reagents, demonstrating its applicability to a variety of analytes and reagents. The derivatization reaction can be directly carried out in neat samples, and after derivatization the samples can be immediately sent to the LC-MS/MS instrument for analysis. These advantages facilitate a one-step sample preparation procedure that can be completed in less than one hour, allowing for a "derivatize & shoot" lab workflow. The derivatization method was applied to establish an LC-MS/MS assay for the quantitation of THC in human breath samples. The derivatization conditions were studied in this application, including the effects of acidity, organic solvent, and diazonium concentration in the reaction. The THC derivatization assay was validated and achieved a limit of quantitation (LOQ) of 0.50 pg/ml using either of the two regio-isomers of the azo-derivative of THC (THC-DRV). To prove that the derivatization method has compatibility with complex-matrix samples, a THC derivatization assay for serum samples was established, in which the azo coupling reaction was directly carried out in crude protein-precipitated supernatants. An LOQ of 5.0 pg/ml was achieved. In addition, excellent correlation between THC derivatization and non-derivatization assays was found in the analysis of whole blood samples. (C) 2019 Elsevier B.V. All rights reserved.
机译：报道了一种基于偶氮偶联的衍生化方法，用于高灵敏度液相色谱 - 串联质谱（LC-MS / MS）定量四氢甘油（THC）和其他芳族化合物，即酚和胺。通过将重氮偶联到分析物的偶氮偶联，它产生衍生化的分析物，其具有增强的电离效率并导致串联质谱中的高响应片段。使用三种不同的重氮盐作为衍生化试剂将衍生化方法应用于六种典型的芳族化合物，证明了其对各种分析物和试剂的适用性。衍生化反应可以直接在整齐的样品中进行，并且在衍生化之后，可以立即将样品发送到LC-MS / MS仪器进行分析。这些优点有助于一步的样品制备程序，可以在不到一小时内完成，允许“衍生和拍摄”实验室工作流程。施用衍生化方法以建立用于定量人类呼吸样品中的LC-MS / MS测定。在本申请中研究了衍生化条件，包括酸度，有机溶剂和重氮浓度在反应中的影响。验证了THC衍生化测定并使用THC（THC-DRV）的偶氮衍生物中的两种测定异构体中的任一种，实现了0.50pg / ml的定量（LOQ）的极限。为了证明衍生化方法具有与复合基质样品的相容性，建立了血清样品的THC衍生化测定，其中偶氮偶联反应直接在粗蛋白质沉淀的上清液中进行。实现了5.0 pg / ml的LOQ。此外，在全血样品的分析中发现了THC衍生化与非衍生化测定之间的优异相关性。 （c）2019 Elsevier B.v.保留所有权利。

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